Sensitive spectrophotometric determination of La(III) with 1-(2-pyridylazo)-2-naphthol

A simple and sensitive method for spectrophotometric determination of lanthanum has been developed. At pH 9.6, in presence of 50% ethanol, lanthanum reacts with 1-(-2-pyridylazo)-2-naphthol (PAN) to form a red complex which has two absorption maxima, at 545 and 510 nm. The molar absorptivity at 545 nm is 0.55 × 10⁴ liters · mol^?1 cm^?1. On the other hand, lanthanum reacts with PAN in pure ethanol to form a red complex at 530 nm, with high molar absorptivity (8 × 10⁴ liters · mol^?1 cm^?1).     

Pre-concentration of trace amounts of manganese in water samples based on (1-(2-pyridylazo)-2-naphthol) modified magnetic nanoparticles

A simple procedure based on magnetic nanoparticles has been developed for analytical purposes. In this method, 1-(2-pyridylazo)-2-naphthol (PAN)-modified magnetic nanoparticles (MNPs) were used for separation and pre-concentration of manganese(II) ions from aqueous samples. This method combines the use of a solution solvent with separation of magnetic nanoparticles from sample solution using a magnet. The influence of different parameters, such as amount of extractant (PAN) loaded on the nanoparticles, pH of solution, adsorption time, amount of modified nanoparticle, type and amount of eluents for desorption of manganese from magnetic nanoparticles were evaluated. The effect of various cationic and anionic interferences on the percentage recovery of manganese was also studied. Manganese ions were adsorped from a solution at pH 9.5 and desorbed from nanoparticles with 10?mL of DMSO?:?HNO₃ (1?:?1, v/v). The detection limit of the proposed method was found to be 0.11?µg?L^?1. The method was employed to recover and determine the level of manganese in different water samples.     

Spectrophotometric determination of uranium with 1-(2-pyridylazo)-2-naphthol

1-(2-Pyridylazo)-2-naphthol (PAN) rcacts with uranium to form a deep red precipitate in ammoniacal solutions, this can be extracted with chloroform if sodium chloride or sulfate is added and it has a maximum absorption at 560 mμ The color is stable and follows Beer's law. Trace amounts of uranium may be determined in the presence of many metals without prior separation if strong complexing agents, such) as EDTA or cyanide, are added     

Colorimetric determination of zirconium with 1-(2-pyridylazo)-2-naphthol

A method is described for the determination of as little as 50 ppm of zirconium in uranium-fission element alloys and zinc magnesium-uranium-fission element alloys. Zirconium is extracted from a nitric acid-aluminium nitrate medium with dibutyl phosphate in toluene. The uranium co-extracted with the zirconium is removed by scrubbing with hydrochloric acid-ammonium thiocyanate solution. A portion of the organic phase is mixed with pyridine-toluene solution of 1-(2-pyridylazo)-2-naphthol to develop the colour.     

Atomic absorption spectrometric determination of trace zinc in alloys and biological samples after preconcentration with [1-(2-pyridylazo)-2-naphthol] on microcrystalline naphthalene

An atomic absorption spectrometric method for the determination of trace amounts of zinc after adsorption of its [1-(2-pyridylazo)-2-naphthol] complex on microcrystalline naphthalene has been developed. This complex is adsorbed on microcrystalline naphthalene in the pH range 3.5-7.5 from large volumes of aqueous solutions of various alloys and biological samples with a preconcentration factor of 40. After filtration, the solid mass consisting of the zinc complex and naphthalene was dissolved with 5 ml of dimethylformamide and the metal was determined by flame atomic absorption spectrometry. Zinc can alternatively be quantitatively adsorbed on [1-(2-pyridylazo)-2-naphthol]-naphthalene adsorbent packed in a column and determined similarly. About 0.5 ng of zinc can be concentrated in a column from 200 ml of aqueous sample, where its concentration is as low as 2.5 pg ml-1. The calibration curve is linear in the range 0.1-6.5 ng ml-1 in dimethylformamide solution. Eight replicate determinations of 2 ng ml-1 of zinc gave a mean absorbance of 0.145 with a relative standard deviation of 1.5%. The sensitivity for 1% absorption was 0.061 ng ml-1. Various parameters, such as the effect of pH and the interference of a number of metal ions on the determination of zinc, have been studied in detail to optimize the conditions for the determination of zinc in various standard complex materials.     

Spectrofluorimetric determination of Ga(III) with 1-hydroxy-2-carboxyanthraquinone

Summary The fluorescent chelate formed between 1-hydroxy-2-carboxy-anthraquinone and gallium(III) at pH 3.9 has been studied spectrofluorimetrically in an ethanol-water mixture (70/30% V/V). A new method for the fluorimetric determination of gallium(III) is described. The fluorescence is monitored at 580 nm (wavelength of excitation 465 nm) and the range of application of the method is between 50 and 500 ng ml^–1. The stoichiometry of the complex has been found to be 11.

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Spektralfluorimetrische Bestimmung von Ga(III) mit 1-Hydroxy-2-carboxyanthrachinon

Zusammenfassung Ein neues Verfahren zur fluorimetrischen Bestimmung von Ga(III) mit 1-Hydroxy-2-carboxyanthrachinon bei pH 3,9 in wäßrigem Ethanol wurde ausgearbeitet. Die Fluoreszenz wurde bei 580 nm gemessen (Anregung bei 465 nm). Das Verfahren eignet sich für 50–500 ng/ml. Die Zusammensetzung der Komplexverbindung entspricht dem Verhältnis 11.

     

Spectrofluorimetric determination of trace amounts of europium(III) ion with lutetium(III)-sparfloxacin-sodium dodecyl sulfate luminescence enhancement system.

A new luminescence-enhancement system based on complex formation between europium and sparfloxacin in the presence of lutetium in a sodium dodecyl sulfate solution has been discovered. By adding a suitable amount of Lu3+ to the Eu-sparfloxacin-sodium dodecyl sulfate system, the luminescence can be enhanced by approximately 5-fold compared with that of the system without Lu3+. Under the optimum conditions, the luminescence intensity of the system is a linear function of the concentration of europium in the range of 1.0 x 10(-10) - 5.0 x 10(-7) mol L(-1). The detection limit of europium is 2.0 x 10(-13) mol L(-1) (S/N = 3). The system was used for the determination of trace amounts of europium in rare earth samples with satisfactory results.     

Adsorptive stripping voltammetric measurements of trace amounts of platinum(II) and ruthenium(III) in the presence of 1-(2-pyridylazo)-2-naphthol

An extremely sensitive stripping voltammetric procedure for low level measurements of platinum (II, IV) or ruthenium (III, IV) is reported. The method is based on the interfacial accumulation of the platinum (II) or ruthenium (III)-1-(2-pyridylazo)-2-naphthol complex on the surface of a hanging mercury drop electrode, followed by the reduction of the adsorbed complex during the cathodic scan. The peak potential was found to be –0.8 V vs. Ag/AgCl electrode and the reduction current of the adsorbed complex ions of platinum (II) or ruthenium (III) was measured by differential pulse cathodic stripping voltammetry. The optimum experimental conditions were: 1.5×10^–7 mol/l of 1-(2-pyridylazo)-2-naphthol solution of pH 9.3, preconcentration potential of –0.2 V, accumulation time of 3 min and pulse amplitude of 50 mV with 4 mV s^–1 scan rate in the presence of ethanol-water (30% v/v) — sodium sulphate (0.5 mol/l). Linear response up to 6.4 × 10^–8 and 5.1 × 10^–8 mol/l and a relative standard deviation (at 1.2×10^–8 mol/l) of 2.4 and 1.6% (n=5) for platinum (II) and ruthenium (III) respectively were obtained. The detection limits of platinum and ruthenium were 3.2×10^–10 and 4.1×10^–10 mol/l, respectively. The electronic spectra of the Pt(II) — PAN and Ru(III) — PAN complexes were measured at pH 9.3 and the stoichiometric ratios of the complexes formed were obtained by the molar ratio method. The effects of some interfering ions on the proposed procedure were critically investigated. The method was found suitable for the sub-microdetermination of ruthenium (IV) and platinum (IV) after their reduction to ruthenium (III) and platinum (II) with sulphur dioxide in acid media. The applicability of the method for the analysis of binary mixtures of ruthenium (III) and (IV) or platinum (II) and (IV) has also been carried out successfully. The method is simple, rapid, precise, and promising for the determination of the tested metal ions at micro-molar concentration level.     

Enhanced spectrophotometric determination of nicotinic acid in a sodium dodecyl sulphate micellar medium

The spectrophotometric determination of pyridine and pyridine derivatives by means of the K?nig reaction was studied in micellar media of sodium dodecyl sulphate (SDS), N-cetylpyridinium chloride and Triton X-100. The sensitivity was largely increased in SDS micellar medium. The attack of the pyridine ring with cyanogen bromide to produce a glutaconic aldehyde was not affected by the presence of SDS, but the yield of the coupling reaction with an arylamine to produce a polymethine dye was largely increased. In the SDS micellar medium, aniline was superior to other coupling reagents. The limits of detection (LODs) were 6 x 10(-7), 1 x 10(-6) and 5 x 10(-7)M for pyridine, pyrrol-ylmethylpyridine and nicotinic acid, respectively, and the reproducibility for 2 x 10(-5)M solutions was ca. 2%. In the absence of SDS, the LODs were 3 x 10(-6), 3 x 10(-6) and 9 x 10(-6)M, respectively, and the reproducibility was ca. 3.5%. Application was made to the determination of nicotinic acid in pharmaceuticals.     

Spectrofluorimetric determination of carbaryl and 1-naphthol in micellar media

The interaction of 1-naphthol-N-methyl-carbamate (carbaryl) and its degradation product, 1-naphthol, with the surfactant hexadecyl-trimethylammonium bromide has been studied. The micellar medium allows the direct spectrofluorimetric determination of carbaryl, with 6.2 ng/ml as detection limit in acidic medium, or indirectly, after hydrolysis, as 1-naphthol at pH 11.0 or pH 3.0 with detection limits of 0.4 and 1.6 ng/ml, respectively. The recoveries of carbaryl and 1-naphthol from natural waters are acceptable.     

Spectrophotometric determination of cobalt with 1-(2-pyridylazo)-2-naphthol and surfactants

A simple and highly selective spectrophotometric method for the determination of cobalt based upon the rapid reaction with PAN in the presence of surfactants and minute amounts of ammonium persulphate at pH 5.0 is described. The cobalt(III) chelate is made water-soluble by a neutral surfactant. Triton X-100, combined with sodium dodecylbenzene sulphonate (DBS). Iron(III), bismuth, tin(IV) and aluminium are masked with oxalate or citrate. Iron(II) must be absent. The other metal-PAN chelates, except that of nickel, are readily decomposed by EDTA. Up to 150 microg of nickel does not interfere. When larger amounts up to 625 microg are present, the absorbance can be corrected by measurements at two wavelengths. In a strongly acid medium (below pH 0.5) the nickel and other metal chelates are completely and instantaneously decomposed, while the cobalt(III) chelate remains unchanged. When, in place of EDTA, several ml of 6M hydrochloric acid are added after the colour development, nickel in quantities up to 1250 microg can be tolerated. A several hundredfold excess of zinc and manganese does not interfere. At 620 nm Beer's law is obeyed over the cobalt concentration range 0.4-3.2 microg/ml. The precision (95% confidence) is +/- 1.0 microg for 100 microg of cobalt. The molar absorptivity is 1.90 x 10(4) l. mole(-1) .cm(-1).     

Spectrophotometric determination of hafnium(IV) with 1-(2-pyridylazo)-2-naphthol

Summary The red complex formed between hafnium(IV) and 1-(2-pyridylazo)-2-naphthol (1 2) at pH 4.0 is used for Spectrophotometric determination of hafnium., the absorbance being measured at 545 nm. Beer's law is obeyed for hafnium concentration of 0.2 to 3.6g per ml. Molar absorptivity is 3.86×10⁴ and Sandell sensitivity is 0.0046g per cm². Hafnium has been determined in the presence of 6-fold amounts of zirconium. The relative standard deviation is ± 1.0%.

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Zusammenfassung Der rote, bei pH 4,0 sich bildende Komplex mit 1-(2-Pyridylazo)-2-naphthol (1 2) dient zur Bestimmung von Hafnium (IV). Seine Extinktion wird bei 545 nm gemessen. Zwischen 0,2 und 3,6g Hf/ml ist das Beersche Gesetz gültig. Hafnium läßt sich in Gegenwart der sechsfachen Menge Zirkonium bestimmen. Die relative Standardabweichung beträgt ± 1,0%.

     

Spectrofluorimetric determination of trace amounts of aluminium with 5-bromo-salicylaldehyde salicyloylhydrazone

The fluorescent reagent 5-bromo-salicylaldehyde salicyloylhydrazone (5-Br-SASH) was synthesized and its ionization constants were established spectrophotometrically. The fluorescent reaction of this reagent with aluminium was studied. Based on this chelation reaction, a spectrofluorimetric method was developed for the determination of aluminium in acetic acid-ammonium acetate buffer solution of pH 5.4. Under these conditions, the A1-5-Br-SASH complex has excitation and emission maxima at 370 and 460 nm, respectively. The linear range of the method is from 0 to 120 ppb and the detection limit is 1.1 ppb of aluminium. The molar ratio of aluminium to the reagent is 1:3. Interferences of other ions were studied. The method was successfully applied to the determination of aluminium in glucose injection and common beverages.     

Spectrophotometric determination of rare earth metals with 1-(2-pyridylazo)-2-naphthol

1-(2-Pyridylazo)-2-naphthol (PAN) reacts very sensitively with rare earth metals to form a deep red precipitate in alkaline solution; this can be extracted with ether, except in the case of lanthanum, cerium and scandium. Absorption maxima occur at 530 and 560 mμ. Traces of rare earth metals may be determined in the presence of many foreign metals.     

Spectrophotometric determination of traces of gallium and indium with 1-(2-pyridylazo)-2-naphthol

1-(2-Pyridylazo)-2-naphthol (PAN) reacts with either gallium or indium at pH 5–6 giving a red complex in an aqueous medium in the presence of N.N-dimethyl-formamide. The maximum absorption of both PAN complexes of gallium and indium in an aqueous solution is at 545 mμ. The gallium-PAN complex shows a characteristic enhancement of color by addition of small amounts of ethers. Based on this selective enhancement reaction, gallium can be determined in the presence of other metals without separation. The results of determining gallium and indium in the presence of each other are reported. Both gallium and indium form M₂(PAN)₃; but in the presence of certain organic solvents, a different gallium complex, Ga(PAN)₅, and the same indium complex, In₂(PAN)₃, are formed. The reaction of PAN with cadmium can be masked by iodide; an example of determining indium in the presence of cadmium is given. The PAN method has a sensitivity of 0.003 μg/cm² for gallium and 0.005μg/cm² for indium and an absorptivity of 24,900 for the Ga-PAN complex and of 24,500 for the In-PAN complex, respectively. The methods have been successfully applied to the determination of both gallium and indium in germanium thin films.     

Spectrophotometric determination of manganese with 1-(2-pyridylazo)-2-naphthol and a non-ionic surfactant

A spectrophotometric method for the determination of trace amounts of manganese with 1-(2-pyridylazo)-2-naphthol (PAN) is described. The method is based on the measurement of absorbance of the manganese—PAN chelate solubilized with a non-ionic surfactant, Triton X-100. No extraction procedure is required in the method proposed. High concentrations of calcium, aluminium and magnesium do not interfere. The presence of up to 10 ppm of lead can be tolerated. Iron, cadmium, zinc, cobalt and nickel can be effectively masked with potassium cyanide. Beer's law is obeyed up to 2 ppm of manganese. The molar absorptivity of the manganese—PAN chelate found was 4.4 × 10⁴ l. mole ⁻¹. cm⁻¹ at 562 nm. The overall stability constant of Mn(PAN)₂ in 0.4% Triton X-100 medium is 10^16.8.     

Preconcentration and determination of Bismuth (III) at a chemically modified electrode containing 1-(2-pyridylazo)-2-naphthol

A chemically modified electrode (CME) containing 1-(2-pyridylazo-2-naphthol is evaluated for its ability to preconcentrate bismuth(III) prior to quantification by voltammetry. The CME approach is shown to be sufficiently sensitive for sub-nanomolar concentrations to be determinable after chemical deposition for 60 sec. Further, when the bismuth is deposited from iodide-containing sulphuric acid media, the discrimination against interference by copper(II) is significantly better than that obtained with conventional stripping analysis. The results obtained for Bi(III)( in an NBS reference solution agree well with the recommended value.     

Determination trace amounts of thallium after separation and preconcentration onto nanoclay loaded with 1-(2-pyridylazo)-2-naphthol as a new sorbent

A procedure has been proposed for the separation and preconcentration of trace amounts of thallium. It is based on the adsorption of thallium ions onto organo nanoclay loaded with 1-(2-pyridylazo)-2-naphthol (PAN). Thallium ions were quantitatively retained on the column in the pH range of 3.5–6.0, whereas quantitative desorption occurs with 5.0?mL of 5% ascorbic acid and thallium was determined by flame atomic absorption spectrometry. Linearity was maintained between 0.66?ng?mL^?1–15.0?µg?mL^?1?in initial solution. Detection limit was 0.2?ng?mL^?1?in initial solution and preconcentration factor was 150. Eight replicate determinations of 2.0?µg?mL^?1 of thallium in final solution gave a relative standard deviation of ±1.48%. Various parameters have been studied, such as the effect of pH, breakthrough volume and interference of a large number of anions and cations and the proposed method was used to determine thallium ions in water and standard samples. Determination of thallium ions in standard sample showed that the proposed method has good accuracy.